CN103265169B - A kind of preparation method of high radioactive nucleus waste vitrification base material - Google Patents
A kind of preparation method of high radioactive nucleus waste vitrification base material Download PDFInfo
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- CN103265169B CN103265169B CN201310197280.5A CN201310197280A CN103265169B CN 103265169 B CN103265169 B CN 103265169B CN 201310197280 A CN201310197280 A CN 201310197280A CN 103265169 B CN103265169 B CN 103265169B
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Abstract
The present invention discloses a kind of preparation method of high radioactive nucleus waste vitrification base material.Containing the high activity liquid waste of higher concentration sulfate radical, because sulphur solubleness in borosilicate melts is lower, make sulphur usually become refuse and contain quantitative limitation factor.Can produce the yellow phase of separation in melting process, serious harm glass solidified body contains and isolates the effect of nucleic.The method regulates useless flint glass chemical constitution, after mixing, and 980 ~ 1100 DEG C of melting 2 ~ 4h, it is made fully to be molten into glass metal, then cast in 700 ~ 850 DEG C of die for molding, put into annealing furnace 400 ~ 550 DEG C insulation 1 ~ 3h, obtain high radioactive nucleus waste vitrification base material.The inventive method with useless flint glass for main raw material, Novel radioactive waste glass curing substrate is prepared by adjustment glass chemistry composition, turn waste into wealth, achieve the recycling of lead glass, glass solidified body is stablized, not easily produce yellow phase in melting process.
Description
Technical field
The invention belongs to Radwastes treatment and dispose field, particularly a kind of preparation method of high radioactive nucleus waste vitrification base material.
Background technology
Nuclear power plants produces some radwastes unavoidably while utilizing nuclear energy power generation, and this kind of refuse has strong destruction to physical environment and organism, and therefore how effectively the key that nuclear waste becomes safe utilization nuclear energy is disposed in process.Solidification nuke rubbish is a kind of important method of process high radioactivity waste material, and current curing technology has ceramic solidification, glass-ceramic solidification, vitrification, prosthetic graft solidification and self propagating high temperature solidification.Ceramic solidification is large to radioelement containing amount in high-level waste, and crystal is strong relative to Vitrea thermostability, but ceramic solidification is strong to the selectivity of radioactive element, and the major part in refuse is "dead", and waste material is very large to ceramic solidification influential effect.Glass-ceramic solidification can effectively solve ceramic solidification Problems existing, and radioactive element major part is cured in lattice, and cold refuse and on a small quantity uncured element in lattice are then cured in glass outer matrix; But this curing mode heat treatment process is comparatively complicated, is still in conceptual phase.After vitrification concentrates evaporate to dryness by nuclear waste with there is the mineral powders suitably formed mix, become airtight storage in special storage field after glassy solids through high temperature sintering.This method has that cured body intensity is high, density good, Stability Analysis of Structures, and the radionuclide be cured leaching yield when water soaking is very low, and thus security is high, and in the country such as American-European-Japanese, oneself becomes one comparatively proven technique application.
Borosilicate glass cured high-level waste is current internationally recognized better method, and the glass solidified body of generation has good chemical durability, and glass melting temperature is at tolerance interval.But for the high activity liquid waste containing higher concentration sulfate radical, because sulphur solubleness in borosilicate melts is lower, make sulphur usually become refuse and contain quantitative limitation factor.Can produce the yellow phase of separation in melting process, serious harm glass solidified body contains and the effect of isolation nucleic, therefore to improve in glass sulphur containing amount for most important the high activity liquid waste vitrification containing high vitriol oil salt.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, a kind of preparation method of high radioactive nucleus waste vitrification base material is provided, the method with useless flint glass for main raw material, Novel radioactive waste glass curing substrate is prepared by adjustment glass chemistry composition, turn waste into wealth, achieve the recycling of lead glass, glass solidified body is stablized, not easily produce yellow phase in melting process.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is as follows:
Step (1). regulate useless flint glass chemical constitution, make each component percentages in useless flint glass as follows: 45 ~ 60 ﹪ SiO
2, 7 ~ 14 ﹪ B
2o
3, 4 ~ 10 ﹪ Al
2o
3, 0.2 ~ 2.5 ﹪ CaO, 6 ~ 13 ﹪ Na
2o, 1 ~ 4 ﹪ Fe
2o
3, 10 ~ 25 ﹪ PbO;
Step (1) can add industrial raw material according to the chemical constitution of useless flint glass, regulates each component percentages in useless flint glass.
Step (2). the useless flint glass after regulating chemical constitution is put into tumbling ball mill ground and mixed evenly, and 980 ~ 1100 DEG C of melting 2 ~ 4h, make it fully be molten into glass metal;
Step (3). glass metal is cast in the mould being preheated to 700 ~ 850 DEG C, is cooled to shaping;
Step (4). after forming composition being put into annealing furnace 400 ~ 550 DEG C insulation 1 ~ 3h, naturally cool to normal temperature, obtain high radioactive nucleus waste vitrification base material.
Described useless flint glass is one or more in CRT panel glass, CRT cone glass, tube glass, radiation shielding glass.
For the high activity liquid waste containing higher concentration sulfate radical, because sulphur solubleness in borosilicate melts is lower, can produce the yellow phase of separation in melting process, serious harm glass solidified body contains and isolates the effect of nucleic.The inventive method with useless flint glass for main raw material, Novel radioactive waste glass curing substrate is prepared by adjustment glass chemistry composition, turn waste into wealth, achieve the recycling of lead glass, glass solidified body is stablized, not easily produce yellow phase in melting process, can realize large-scale promotion application.
Embodiment
Below in conjunction with specific embodiment, the present invention is further analyzed.
Embodiment 1
Step (1). regulate the chemical constitution of black and white television set CRT panel glass, make each component percentages in CRT panel glass as follows: 45 ﹪ SiO
2, 14 ﹪ B
2o
3, 10 ﹪ Al
2o
3, 2.5 ﹪ CaO, 13 ﹪ Na
2o, 4 ﹪ Fe
2o
3, 11.5 ﹪ PbO;
Step (2). the CRT panel glass after regulating chemical constitution is put into tumbling ball mill ground and mixed evenly, and 1100 DEG C of melting 4h, make it fully be molten into glass metal;
Step (3). glass metal is cast in the mould being preheated to 700 DEG C, is cooled to shaping;
Step (4). after forming composition being put into annealing furnace 550 DEG C insulation 1h, naturally cool to normal temperature, obtain high radioactive nucleus waste vitrification base material.
Embodiment 2
Step (1). regulate the chemical constitution of CRT cone glass, make each component percentages in CRT cone glass as follows: 60 ﹪ SiO
2, 7 ﹪ B
2o
3, 4 ﹪ Al
2o
3, 0.2 ﹪ CaO, 6 ﹪ Na
2o, 1 ﹪ Fe
2o
3, 21.8 ﹪ PbO;
Step (2). the CRT cone glass after regulating chemical constitution is put into tumbling ball mill ground and mixed evenly, and 980 DEG C of melting 2h, make it fully be molten into glass metal;
Step (3). glass metal is cast in the mould being preheated to 850 DEG C, is cooled to shaping;
Step (4). after forming composition being put into annealing furnace 400 DEG C insulation 3h, naturally cool to normal temperature, obtain high radioactive nucleus waste vitrification base material.
Embodiment 3
Step (1). regulate the chemical constitution of tube glass, make each component percentages in tube glass as follows: 58.5 ﹪ SiO
2, 9 ﹪ B
2o
3, 6 ﹪ Al
2o
3, 1.5 ﹪ CaO, 12 ﹪ Na
2o, 3 ﹪ Fe
2o
3, 10 ﹪ PbO;
Step (2). the tube glass after regulating chemical constitution is put into tumbling ball mill ground and mixed evenly, and 1000 DEG C of melting 3h, make it fully be molten into glass metal;
Step (3). glass metal is cast in the mould being preheated to 750 DEG C, is cooled to shaping;
Step (4). after forming composition being put into annealing furnace 450 DEG C insulation 2h, naturally cool to normal temperature, obtain high radioactive nucleus waste vitrification base material.
Embodiment 4
Step (1). regulate the chemical constitution of radiation shielding glass, make each component percentages in radiation shielding glass as follows: 54 ﹪ SiO
2, 8 ﹪ B
2o
3, 5.5 ﹪ Al
2o
3, 0.5 ﹪ CaO, 6 ﹪ Na
2o, 1 ﹪ Fe
2o
3, 25 ﹪ PbO;
Step (2). the radiation shielding glass after regulating chemical constitution is put into tumbling ball mill ground and mixed evenly, and 990 DEG C of melting 2.5h, make it fully be molten into glass metal;
Step (3). glass metal is cast in the mould being preheated to 780 DEG C, is cooled to shaping;
Step (4). after forming composition being put into annealing furnace 460 DEG C insulation 2.5h, naturally cool to normal temperature, obtain high radioactive nucleus waste vitrification base material.
Embodiment 5
Step (1). regulate the chemical constitution of colour television set CRT panel glass, make each component percentages in CRT panel glass as follows: 56.8 ﹪ SiO
2, 9.1 ﹪ B
2o
3, 8.8 ﹪ Al
2o
3, 1.6 ﹪ CaO, 8.2 ﹪ Na
2o, 3.5 ﹪ Fe
2o
3, 12 ﹪ PbO;
Step (2). the CRT panel glass after regulating chemical constitution is put into tumbling ball mill ground and mixed evenly, and 1050 DEG C of melting 3h, make it fully be molten into glass metal;
Step (3). glass metal is cast in the mould being preheated to 810 DEG C, is cooled to shaping;
Step (4). after forming composition being put into annealing furnace 520 DEG C insulation 1.5h, naturally cool to normal temperature, obtain high radioactive nucleus waste vitrification base material.
Embodiment 6
Step (1). regulate the chemical constitution of tube glass, make each component percentages in tube glass as follows: 48.6 ﹪ SiO
2, 10.6 ﹪ B
2o
3, 6.4 ﹪ Al
2o
3, 1.8 ﹪ CaO, 7.4 ﹪ Na
2o, 3.2 ﹪ Fe
2o
3, 22 ﹪ PbO;
Step (2). the tube glass after regulating chemical constitution is put into tumbling ball mill ground and mixed evenly, and 1080 DEG C of melting 3.5h, make it fully be molten into glass metal;
Step (3). glass metal is cast in the mould being preheated to 800 DEG C, is cooled to shaping;
Step (4). after forming composition being put into annealing furnace 530 DEG C insulation 2.5h, naturally cool to normal temperature, obtain high radioactive nucleus waste vitrification base material.
Embodiment 7
Step (1). regulate the chemical constitution of colour television set CRT panel glass and CRT cone glass, make each component percentages in colour television set CRT panel glass and CRT cone glass as follows: 48.9 ﹪ SiO
2, 11 ﹪ B
2o
3, 6 ﹪ Al
2o
3, 0.9 ﹪ CaO, 11.7 ﹪ Na
2o, 3.5 ﹪ Fe
2o
3, 18 ﹪ PbO;
Step (2). the colour television set CRT panel glass after adjustment chemical constitution and CRT cone glass are put into tumbling ball mill ground and mixed even, 990 DEG C of melting 2h, make it fully be molten into glass metal;
Step (3). glass metal is cast in the mould being preheated to 800 DEG C, is cooled to shaping;
Step (4). after forming composition being put into annealing furnace 440 DEG C insulation 3h, naturally cool to normal temperature, obtain high radioactive nucleus waste vitrification base material.
Embodiment 8
Step (1). regulate the chemical constitution of black and white television set CRT panel glass, CRT cone glass, tube glass, make each component percentages in black and white television set CRT panel glass, CRT cone glass, tube glass as follows: 49.33 ﹪ SiO
2, 11.4 ﹪ B
2o
3, 9.7 ﹪ Al
2o
3, 0.23 ﹪ CaO, 7.38 ﹪ Na
2o, 1.06 ﹪ Fe
2o
3, 20.9 ﹪ PbO;
Step (2). the black and white television set CRT panel glass after adjustment chemical constitution, CRT cone glass, tube glass are put into tumbling ball mill ground and mixed evenly, and 1010 DEG C of melting 3.2h, make it fully be molten into glass metal;
Step (3). glass metal is cast in the mould being preheated to 805 DEG C, is cooled to shaping;
Step (4). after forming composition being put into annealing furnace 490 DEG C insulation 2.5h, naturally cool to normal temperature, obtain high radioactive nucleus waste vitrification base material.
Above-described embodiment 1 ~ 8 step (1) can add industrial raw material according to the chemical constitution of useless flint glass, regulates each component percentages in useless flint glass.
Above-described embodiment is not that the present invention is not limited only to above-described embodiment for restriction of the present invention, as long as meet application claims, all belongs to protection scope of the present invention.
Claims (2)
1. a preparation method for high radioactive nucleus waste vitrification base material, is characterized in that the method comprises the following steps:
Step (1). regulate useless flint glass chemical constitution, make each component percentages in useless flint glass as follows: 45 ~ 60 ﹪ SiO
2, 7 ~ 14 ﹪ B
2o
3, 4 ~ 10 ﹪ Al
2o
3, 0.2 ~ 2.5 ﹪ CaO, 6 ~ 13 ﹪ Na
2o, 1 ~ 4 ﹪ Fe
2o
3, 10 ~ 25 ﹪ PbO;
Step (1) adds industrial raw material according to the chemical constitution of useless flint glass, regulates each component percentages in useless flint glass;
Step (2). the useless flint glass after regulating chemical constitution is put into tumbling ball mill ground and mixed evenly, and 980 ~ 1100 DEG C of melting 2 ~ 4h, make it fully be molten into glass metal;
Step (3). glass metal is cast in the mould being preheated to 700 ~ 850 DEG C, is cooled to shaping;
Step (4). after forming composition being put into annealing furnace 400 ~ 550 DEG C insulation 1 ~ 3h, naturally cool to normal temperature, obtain high radioactive nucleus waste vitrification base material.
2. the preparation method of a kind of high radioactive nucleus waste vitrification base material as claimed in claim 1, is characterized in that described useless flint glass is one or more in CRT panel glass, CRT cone glass, tube glass, radiation shielding glass.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310781B (en) * | 2014-10-11 | 2017-07-04 | 中国核动力研究设计院 | A kind of glass basis composition and glass solidified body prepared therefrom for middle low-level radioactivity combustible waste burning ash |
| CN104658627B (en) * | 2015-02-02 | 2017-09-01 | 中广核研究院有限公司 | A kind of firming body handled for low and intermediate level radioac glass solidification and method |
| CN104681115B (en) * | 2015-02-28 | 2017-05-24 | 中广核研究院有限公司 | Glass solidifying body protection system |
| CN104810072B (en) * | 2015-03-09 | 2017-06-30 | 西南科技大学 | A kind of preparation method of sulfur-bearing high activity liquid waste glass ceramics curing substrate |
| CN109994240B (en) * | 2017-12-31 | 2022-10-28 | 中国人民解放军63653部队 | Method for reducing solidifying and melting temperature of radionuclide-polluted sandy soil glass |
| CN108417287B (en) * | 2018-02-08 | 2020-04-21 | 武汉理工大学 | Method for co-processing waste lead-containing CRT glass and high-level radioactive waste liquid |
| CN109273130B (en) * | 2018-08-07 | 2022-03-29 | 西南科技大学 | Preparation method of high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body |
| CN109775994B (en) * | 2019-03-26 | 2021-08-31 | 西南科技大学 | Low-temperature curing method for glass ceramic coated with silver silica gel |
| CN109748509B (en) * | 2019-03-26 | 2021-08-31 | 西南科技大学 | Low-temperature curing method of borate glass ceramic coated with silver silica gel |
| CN112624608B (en) * | 2020-12-18 | 2022-09-06 | 中国建筑材料科学研究总院有限公司 | Borosilicate glass curing substrate and preparation method and application thereof |
| CN115818927B (en) * | 2022-11-11 | 2024-07-09 | 中国科学技术大学 | Method for eliminating molybdate yellow phase in nuclear waste glass solidified body |
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| JPS5580735A (en) * | 1978-12-07 | 1980-06-18 | Nippon Electric Glass Co Ltd | Solidification treating method for high level radioactive waste |
| JPS6082895A (en) * | 1983-10-13 | 1985-05-11 | 株式会社神戸製鋼所 | Melting solidifying treating method of sodium sulfate |
| CN101826376B (en) * | 2010-05-07 | 2013-07-31 | 西南科技大学 | Preparation method of vitrification substrate for radioactive nuclear waste |
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Effective date of registration: 20201123 Address after: 226002 Jiangsu Province, Nantong city Gangzha District happiness street jiangba village community group 2 Patentee after: NANTONG DRAYSON COMPOSITES Co.,Ltd. Address before: 310016 room 3003-1, building 1, Gaode land center, Jianggan District, Hangzhou City, Zhejiang Province Patentee before: Zhejiang Zhiduo Network Technology Co.,Ltd. |
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